UPLC-MS/MS法检测中成药及保健品中非法添加降糖及降脂类化学药物

Determination of Hypoglycemic and Lipid-lowering Drugs Illegally Added to Chinese Patent Medicines and Dietary Supplements by UPLC-MS/MS

目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时检测中成药及保健品中非法添加的降糖及降脂类化学成分。方法:样品经甲醇超声处理后,采用Waters Acquity BEH-C18(2.1 mm×100 mm,1.7μm)色谱柱分离,以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱,流速为0.3 ml·min-1;采用三重四极杆串联质谱(QQQ)作为检测器,电喷雾离子源(ESI),正负离子模式、多反应监测(MRM)模式检测14种降糖降脂类药物,以保留时间、碎片离子比对和峰面积进行定性定量分析。结果:14种降糖、降脂类药物在0.1~500 ng·ml-1范围内呈良好的线性关系,相关系数均大于0.996,检出限为0.000 2~3.940 6ng·ml-1,3个浓度水平回收率均在80%~120%之间。结论:本实验方法准确、灵敏、高效、便捷,可用于降糖、降脂类中成药及保健品中非法添加药物的定性及定量检测。

Objective:To establish a UPLC-MS/MS method for the determination of hypoglycemic and lipid-lowering compounds illegally added to Chinese patent medicines and dietary supplements.Methods:After ultrasonic extracted by methanol,the samples were separated on a Waters Acquity BEH-C18(2.1 mm×100 mm,1.7μm)column with 0.1%formic acid and acetonitrile as the mobile phase.The flow rate was 0.3 ml·min-1.Triple quadrupole mass analyzer(QQQ),electrospray ionization(ESI),positive and negative ion scanning,and multiple reactions monitoring(MRM)mode were used to analyze 14 kinds of hypoglycemic and lipid-lowering drugs.The qualitative analysis and quantitative analysis were based on the retention time,fragment ions and peak area.Results:The 14 kinds of hypoglycemic and lipid-lowering drugs showed good linear relationships within the range of 0.1-500 ng·ml-1 with the correlation coefficients above 0.996.The detection limit was 0.000 2-3.940 6 ng·ml-1.The recoveries were within the range of 80%-120%.Conclusion:The established method is accurate,sensitive,efficient and convenient.It can be used for the qualitative and quantitative determination of hypoglycemic and lipid-lowering drugs illegally added to the Chinese patent medicines and dietary supplements.